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[Reprinted from thf Journal of the American, Chemical Society, 
Vol. XVIII., No. 2. February 1S96.] 



THE USE OF THE CALORIMETER IN DETECTING ADUL- 
TERATIONS OF BUTTER AND LARD. 1 

By E- A. de Schweinitz and James A. Emery. 
i\ • 

Received January 3, 1896. 

WHILE engaged in a study of the comparative value of 
butters and oleomargarines, it occurred to one of us 
that possibly the determinations of their respective heats of 
combustion might be useful if taken in connection with other 
data. Prof. Atwater, who has for some time been conducting 
experiments with an improved calorimeter, very kindly con- 
sented to burn such samples as might be sent to him. The first 
results were so interesting that it occurred to us at once that 
this method might be useful in detecting the adulteration of but- 
ter with oleomargarine, and also perhaps in distinguishing 
between lards of different sources and compound lards. Accord- 
ingly, some specially selected samples of which duplicates were 
kept in our laboratory, were sent to Prof. Atwater, and in the 
case of the butters and oleomargarines the results confirmed our 
first suppositions. In the use of the lards, however, the results 
were not so sharply distinctive, but taken in conjunction with 
other analytical data will prove, as we will endeavor to show, 

1 Read at the Cleveland meeting, Dec. 31, 1895. 



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CALORIMETER FOR BUTTER AND LARD. 3 

exceedingly useful. The samples were forwarded to Prof. 
Atwater, prepared for combustion, without any description of 
their character being given except that they were fats. It is 
well understood that the estimation of the calories is of consider- 
able use in a determination of the molecular weights of complex 
molecules and the results which we will report will serve to 
show, we think, practical application of the use of the bomb 
calorimeter. 

This is best seen by a study of the following tables, which 
give in detail the examinations that are ordinarily made for 
oleomargarine and butter (Table I.), and accompanying these 
examinations the calories per gram. The samples were pre- 
pared for these latter determinations by washing, melting, filter- 
ing, and drying the samples at ioo° C. 

The figures given by different authorities for butter fat, vary 
slightly. Stohman gives the heat equivalent as determined by 
the potassium chlorate method as 9.192 small calories per gram, 
while by the oxygen method it was 9.231 calories per gram. 
The three samples of pure butter burned were from the follow- 
ing sources : No. 28, the best butter used by Armour & Co., in 
the manufacture of butterine. No. 26, was Elgin Creamery 
butter, and No. 27, obtained from a Virginia gentleman, who 
sent it as a sample of the best butter made on his place. Nos. 
31, 32, and 33, were mixtures of Elgin butter and oleomargarine. 
The figures obtained for butter fat are a little higher than those 
Stohman gives for pure butter. 

Table II The steady increase in the calories of the mixtures 

is in proportion to the amount of oleomargarine added to the 

butter and this taken in conjunction with the iodine number 

gives additional confirmatory evidence of the character of the 

sample. 

TABLE II. 

Mixture Composed of Definite Proportions of Elgin and Wood- 

LAWN NO. 2 3 . 



Sample, 
f E and \ W, No. 2 3 . 
\ Fand |W, No. 2 3 . 
JEand |W, No. 2 3 . 



Actual 

iodine 

equivalent. 


Theoretical 

iodine 
equivalent. 


Actual 

combustion 

calories 

per gram. 


Theoretical 
combustion 

calories 
per gram. 


• 43-90 


43-76 


9-39 1 


9.412 


• 48.01 


49-77 


9.416 


9.498 


• 55.40 


55.78 


9.491 


9.584 



4 E. A. DE SCHWEINITZ AND JAMES A. EMERY. 

The theoretical calories per gram for the above mixtures as 
compared with those found are, 

Theory. Found. 

No. 31 9-412 9-391 

No. 32 9.498 9416 

No. 33 9.584 9.491 

The actual combustion of the sample containing a small 
admixture of oleomargarine falls a little lower than theory 
requires, but is sufficiently high to indicate at once that there is 
adulteration of the normal butter. The other two samples give 
results still more distinctive and characteristic. The determina- 
tion of the calories would be sufficient, therefore, to detect oleo- 
margarine. If not relied upon entirely it still furnishes very 
satisfactory evidence. One point to which attention should be 
called is the exceedingly low temperature at which the oleomar- 
garines melted. They were purchased at the end of winter and 
probably made to suit the winter trade. If left in an open dish 
in the laboratory for a few hours they became soft and semi- 
fluid. 

In the case of the lards from various sources the results are 
somewhat different and are not so distinctive as compared with 
compound lard, as the butter and oleomargarine. (Table III.) 
Still even here the determination of the calories taken in con- 
junction with other determinations, as the iodine absorption, 
will also be of use. Should the determination of the calories 
show a low figure one could conclude that the lard was either a 
compound or a lard from the caul, intestines, or head of the ani- 
mals, while the determination of the iodine number and cotton- 
seed-oil test, would show at once whether the sample was a lard 
or a compound lard. The error of experiment in calorimetric 
work is usually counted at twenty-five calories per gram, but by 
careful work can be made less and a number of experiments in 
the same line as the above, would probably give data that would 
make the determination of the calories of still more practical 
value. 



E. A. DE SCHWEINITZ AND JAMES A. EMERY. 5 

TABLE III. 
Analvses of Specimens from Armour & Co. 

Combustion Cotton-seed oil, 
Melting Iodine calories Bechi's 

Quality. point, equivalent, per gram. test. 

Lard, leaf 56.85 9.621 none. 

" caul fat 40.0 58.61 9-573 Slightly darken 

" intestinal fat 40. 7 54.74 9.581 " " 

" heads 29.5 68.79 9-5°3 None. 

" mixture of 

all fats 63.86 9.654 " 

" trimmings 65.57 9.606 " 

" compound, 

1st grade 86.18 9.583 Purple brown. 

" compound, 

2nd grade 86.57 9.530 " " 

shield 61.01 9.598 None. 

" special pure 37. 5 63.63 9.617 " 

In a recent number of this Journal, September, 1895, Wesson 
has very carefully reviewed the subject of the determination of 
the iodine absorption number in pure and compound lards, 
claiming that the figures heretofore given for pure lard were too 
low for the present methods of manufacture. This point also 
came up for incidental consideration in connection with our 
other examinations. We secured two sets of samples from Chi- 
cago, one sent direct from Armour & Co. (Table III), with the 
statement that the samples were what the names indicated. The 
other set of samples was accompanied by a certificate from the 
inspector testifying to the character of the material as forwarded. 

TABLE IV. 
Analyses of Lards from Armour & Co. 

Iodine Cotton-seed oil, 

Quality. equivalent. Bechi's test. 

Leaf 55-6o No reaction. 

Caul fat 58.08 

Intestinal fat 52.94 ' " 

Heads 62.36 " " 

Trimmings 61.58 " " 

Special pure 6087 " " 

Foreign shield 58.62 " " 

Exp. Ref. Comp 69.79 Purple black. 

Prime steam 65.97 No reaction. 

Dom. comp. 74-53 Purple black. 



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III 
000 891 420 5 



6 CALORIMETER FOR BUTTER AND LARD. 

TABLE V. 

Iodine Cotton-seed-oil, Combustion calo- 

Satnple. equivalent. Bechi's test. ries per gram. 

Lard No. 5 58.98 

Lard Plains 50.49 9.606 

Cottolene 90.89 Purple black. 

In addition two other samples of lard, one from Virginia, the 

other from Rhode Island, were examined. The samples sent 

with the inspectors' certificate were freshly made, while the 

other set was older material. There is a decided variation in 

the iodine equivalent and in deciding upon the character of the 

lard, the origin of the sample should undoubtedly be taken into 

consideration. As this is often not possible a check upon the 

other results may be secured by the determination of the calories. 

B ' :>'! Ti 1 . Laboratory. Washi w?ok, >. C 
December 14th, 1895. 

Discussion. — Mr. A. H. Sabin : I am very decidedly of the 
opinion that in investigations as to fats and oils, conclusive and 
satisfactory results can only be obtained by a comparison of 
methods. Such a method as this seems to me to be of a good 
deal of practical value because it is definite and positive. We 
make a combustion in this way and get some results which can 
be depended upon, and which can be verified ; and the condi- 
tions are not difficult to duplicate. While I doubt if such a 
method will be of permanent value, because in such matters the 
ingenuity of the manufacturer is always pitted against the skill 
of the analyst, such a method always has weight, and must be 
taken in conjunction with other methods which also have weight 
and which also by themselves are not conclusive, but which 
have cumulative effect. I am certain that in regard to the 
vegetable fats it is only possible to arrive at just conclusions 
by a comparison of methods. 



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